CN107523833B - A kind of metallographic etching agent and its application in display steel in terms of carbide, crystal boundary - Google Patents
A kind of metallographic etching agent and its application in display steel in terms of carbide, crystal boundary Download PDFInfo
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- CN107523833B CN107523833B CN201710724755.XA CN201710724755A CN107523833B CN 107523833 B CN107523833 B CN 107523833B CN 201710724755 A CN201710724755 A CN 201710724755A CN 107523833 B CN107523833 B CN 107523833B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/28—Acidic compositions for etching iron group metals
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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Abstract
The present invention relates to a kind of metallographic etching agent and its applications in display steel in terms of carbide, crystal boundary, belong to the chemical method lithographic technique field of metal material.Metallographic etching agent of the invention is made of the raw material of picric acid, surfactant A, surfactant B and following volumes number: 3~5 parts of acetic anhydride, 60~75 parts of methanol and 20~40 parts of water；Every 1ml methanol is corresponding to use 0.2~0.4g picric acid；The surfactant A is neopelex；The surfactant B is at least one of sodium sulfate of polyethenoxy ether of fatty alcohol, dodecanolyacylamine, nonylphenol polyoxyethylene ether；The mass ratio of the picric acid, surfactant A and surfactant B is 1~8:3~6:0.2~0.5.It can realize that carbide and crystal boundary pattern quickly, clearly, are really shown in steel using metallographic etching agent of the invention.
Description
Technical field
The present invention relates to a kind of metallographic etching agent and its applications in display steel in terms of carbide, crystal boundary, belong to gold
Belong to the chemical method lithographic technique field of material.
Background technique
As industrial technology is constantly progressive, the Service Environment of mould steel becomes increasingly harsher, this proposes mould steel
Higher performance requirement.Studies have shown that the reinforcing of mould steel is a variety of strengthening mechanisms such as refined crystalline strengthening and Carbide Precipitation reinforcing
The result that comprehensive function is overlapped mutually.Therefore, how to obtain distribution of carbides situation and the size of crystal grain in steel is that research and development are high
One of the main path of performance mould steel.
In the prior art, (the influence Wu Xiao of the low-temperature treatment to carbide in 3CrMoCoWV hot die steel such as Wu Xiaochun
Spring etc., mechanical engineering material, the phase of volume 2012,36 10,70-73 pages of) use 4%HNO3Alcoholic solution is to 3CrMoCoWV Forming Die
Corroded in tool steel, obtains the distribution of carbides situation in steel.(novel cold work die steel SDC99 performance, the Li Chen such as Li Chenhui
Brightness etc., material heat treatment journal, the phase of volume 2013,34 4,80-84 pages) use 4%HNO3Alcoholic solution to Cr2MoV mould steel into
It has gone corrosion, has observed distribution of carbides situation in steel.But 4%HNO3Alcohol corrosive liquid does not generate corrosion to the crystal boundary of mould steel
Behavior, it is necessary to again sample preparation corrosion crystal boundary just can the grain size size to steel be measured.Application publication number is
The Chinese invention patent application of CN102465296A discloses a kind of metallographic etching agent, is made of hydrochloric acid, nitric acid, acetic acid and water,
The metallographic etching agent is suitable for G3 steel alloy, but Corrosion results only have effect to crystal boundary, and is then stale-proof to carbide in steel
Erosion.Application publication number is that the Chinese invention patent application of CN103628062A discloses a kind of corrosive agent, by below according to quality
The group of percentages is grouped as: picric acid: 8~15%, neopelex: 8~12%, copper: 0~1.5% remaining be
Water corrodes steel using the corrosive agent, can show the crystal boundary in steel, but cannot corrode the carbide in steel.In order to
It reaches while observing carbide in steel and need a kind of crystal boundary and base that can corrode steel simultaneously in crystal boundary and transgranular distribution situation
Body is to show the metallographic etching agent of carbide and crystal boundary.
Summary of the invention
The object of the present invention is to provide a kind of metallographics that can corrode carbide and crystal boundary in mould steel or ordinary carbon steel simultaneously
Corrosive agent.
The present invention also provides a kind of application of above-mentioned metallographic etching agent in display steel in terms of carbide, crystal boundary.
In order to achieve the goal above, technical solution used by metallographic etching agent of the invention is:
Metallographic etching agent is made of the raw material of picric acid, surfactant A, surfactant B and following volumes number:
3~5 parts of acetic anhydride, 60~75 parts of methanol and 20~40 parts of water；Every 1ml methanol is corresponding to use 0.2~0.4g picric acid；The table
Face activating agent A is neopelex；The surfactant B is sodium sulfate of polyethenoxy ether of fatty alcohol, dodecyl
At least one of alkylolamides, nonylphenol polyoxyethylene ether；The mass ratio of the picric acid, surfactant A and surfactant B
For 1~8:3~6:0.2~0.5.
The surfactant B is sodium sulfate of polyethenoxy ether of fatty alcohol, dodecanolyacylamine and polyoxyethylene nonyl phenyl second
The mixture of alkene ether.Sodium sulfate of polyethenoxy ether of fatty alcohol, dodecanolyacylamine and polyoxyethylene nonyl phenyl second in the mixture
The mass ratio of alkene ether is 0~5:0~10:0~10.
After metallographic etching agent corrodes mould steel, the hydrophobic group of surfactant contacts matrix, carbide,
It is protected to continue to be corroded by metallographic etching agent；In addition, surfactant can also abolish protection of the grain boundaries hydrophobic group to material,
And continue that crystal boundary is allowed to be corroded.
The raw material of metallographic etching agent of the invention can be to avoid the acid mistake of metallographic etching agent using picric acid and acetic anhydride
By force, while the hydrionic ionization of the picric acid in metallographic etching agent obtained and acetic acid is played the role of mutually promoting, in turn
The acidity of metallographic etching agent is enhanced, and can be excessively weak to avoid acidity, can be used to show that carbide is simultaneously in mould steel
Corrode crystal boundary out.It can realize that carbide and crystal boundary pattern are quickly, clearly, really in mould steel using metallographic etching agent of the invention
Display.
The preparation method of metallographic etching agent of the invention, comprising the following steps: each raw material for taking formula ratio, by picric acid,
Acetic anhydride and methanol be added to the water it is uniformly mixed, then add remaining raw material be uniformly mixed to get.
Technical program of the present invention also lies in: application of the above-mentioned metallographic etching agent in display steel in terms of carbide, crystal boundary.
Application of the metallographic etching agent in display steel in terms of carbide, crystal boundary: the following steps are included: will have throwing
The steel of smooth surface immerse corrosion to burnishing surface in metallographic etching agent and change colour, and are cleaned, are dried after taking-up.
The discoloration refers to that burnishing surface becomes silver color, grey or silver gray.
The burnishing surface of steel is by the way that mould steel is polished, polishes generation.
Preferably, metallographic etching agent is heated to after 60~100 DEG C again corroding steel immersion metallographic etchant.Steel
The time that material corrodes in 60~100 DEG C of metallographic etching agent is 3~10s.
The heating is heated using alcolhol burner, magnetic stirring apparatus or other heating methods.Using magnetic stirring apparatus into
When row heating, the power of magnetic stirring apparatus is 3kw.
The neutral liquid that the cleaning uses.The neutral liquid is one of alcohol, acetone, deionized water.
The drying is to spontaneously dry under drying or normal pressure.The temperature of the drying be 60~80 DEG C, the time be 10~
30s。
Etching pit of the invention in display mould steel in terms of carbide, crystal boundary in application, can be to brilliant in steel
Boundary and matrix are corroded, and can show the size of the precipitation position and crystal grain of carbide after corrosion in microscopic structure simultaneously.It will
Metallographic etching agent of the invention is for when showing carbide in mould steel, crystal boundary, reaction speed to be moderate, and etching time is easy to slap
Control, corrosive agent is relatively stable, and reproducibility is preferable.
Detailed description of the invention
Fig. 1 is that the metallographic etching agent of embodiment 1 schemes the SEM of the burnishing surface after Cr12MoV steel corrosion；
Fig. 2 is that the metallographic etching agent of embodiment 2 schemes the SEM of the burnishing surface after 4Cr5MoSiV1 steel corrosion.
Specific embodiment
Below in conjunction with specific embodiment, further description of the technical solution of the present invention.
Picric acid employed in specific embodiment, acetic anhydride and methanol are that analysis is pure.
Embodiment 1
The metallographic etching agent of the present embodiment, by picric acid, surfactant A, surfactant B and following volumes number
Raw material is made: 5 parts of acetic anhydride, 60 parts of methanol and 20 parts of water；Every 1ml methanol is corresponding to use 0.3g picric acid；The surface-active
Agent A is neopelex；The surfactant B is the mixing of dodecanolyacylamine and nonylphenol polyoxyethylene ether
The mass ratio of object, dodecanolyacylamine and nonylphenol polyoxyethylene ether is 5:5；The picric acid, surfactant A and surface
The mass ratio of activating agent B is 5:4:0.2.
The preparation method of the metallographic etching agent of the present embodiment, comprising the following steps: each raw material for taking formula ratio, by picric acid
With acetic anhydride be added methanol in be uniformly mixed, then add remaining raw material be uniformly mixed to get.
Application of the metallographic etching agent of the present embodiment in display steel in terms of carbide, crystal boundary, comprising the following steps: will
The size that wire cutting obtains is that the Cr12MoV mould steel of 30 × 30 × 20mm is polished, polishes to form the mould with burnishing surface
Has steel sample to be corroded；Use DS-101S heat collecting type constant-temperature heating magnetic stirring apparatus under the power of 3kw by metallographic etching agent again
80 DEG C are heated to, then immerses mould steel sample to be corroded in metallographic etching agent, 10s is corroded to burnishing surface, at this time burnishing surface
It in silver gray, takes out, is then in neutrality with alcohol washes to cleaning solution, then with filter paper gently wiped clean, and blown with dryer
It is dry.
With the burnishing surface of the Cr12MoV mould steel in scanning electron microscopic observation the present embodiment after excessive erosion, as a result such as Fig. 1 institute
Show.As shown in Figure 1, white particle is the carbide in Cr12MoV mould steel, and wherein carbide mainly has VC, Cr7C3, Cr23C6,
Mo2C etc. is constituted, and tiny curve is then the crystal boundary in Cr12MoV mould steel.
Embodiment 2
The metallographic etching agent of the present embodiment, by picric acid, surfactant A, surfactant B and following volumes number
Raw material is made: 3 parts of acetic anhydride, 75 parts of methanol and 40 parts of water；Every 1ml methanol is corresponding to use 0.4g picric acid；The surface-active
Agent A is neopelex；The surfactant B is sodium sulfate of polyethenoxy ether of fatty alcohol, dodecanolyacylamine
With the mixture of nonylphenol polyoxyethylene ether, sodium sulfate of polyethenoxy ether of fatty alcohol, dodecanolyacylamine and polyoxyethylene nonyl phenyl
The mass ratio of vinethene is 5:0.1:10；The mass ratio of the picric acid, surfactant A and surfactant B is 8:6:
0.5。
The preparation method is the same as that of Example 1 for the metallographic etching agent of the present embodiment.
Application of the metallographic etching agent of the present embodiment in display steel in terms of carbide, crystal boundary, comprising the following steps: will
The 4Cr5MoSiV1 mould steel that the size that wire cutting obtains is 30 × 30 × 20mm (passes through+580 DEG C × 20min of 1020 DEG C of quenchings
Double tempering processing) it polished, polish the mould steel sample to be corroded to be formed with burnishing surface；DS-101S thermal-arrest is used again
Metallographic etching agent is heated to 100 DEG C under the power of 3kw by formula constant-temperature heating magnetic stirring apparatus, then by mould steel sample to be corroded
Product immerse in metallographic etching agent, corrode 3s to burnishing surface, and burnishing surface is in silver gray at this time, take out, are then cleaned with acetone to clear
Washing lotion is in neutrality, then with filter paper gently wiped clean, is then spontaneously dried under normal pressure.
With the burnishing surface of the 4Cr5MoSiV1 mould steel in scanning electron microscopic observation the present embodiment after excessive erosion, as a result such as scheme
Shown in 2.The tiny globular carbide that acicular martensite, tempering are precipitated in burnishing surface microscopic structure after corroding as seen from Figure 2,
And the crystal boundary that tiny curve is shown.
Embodiment 3
The metallographic etching agent of the present embodiment, by picric acid, surfactant A, surfactant B and following volumes number
Raw material is made: 4 parts of acetic anhydride, 70 parts of methanol and 30 parts of water；Every 1ml methanol is corresponding to use 0.3g picric acid；The surface-active
Agent A is neopelex；The surfactant B is sodium sulfate of polyethenoxy ether of fatty alcohol, dodecanolyacylamine
With the mixture of nonylphenol polyoxyethylene ether, sodium sulfate of polyethenoxy ether of fatty alcohol, dodecanolyacylamine and polyoxyethylene nonyl phenyl
The mass ratio of vinethene is 5:10:1；The mass ratio of the picric acid, surfactant A and surfactant B is 8:4:0.3.
The preparation method is the same as that of Example 1 for the metallographic etching agent of the present embodiment.
Application of the metallographic etching agent of the present embodiment in display steel in terms of carbide, crystal boundary, comprising the following steps: will
The size that wire cutting obtains is that the 4Cr5MoSiV1 mould steel of 30 × 30 × 20mm is polished, polishes to be formed with burnishing surface
Mould steel sample to be corroded；Use DS-101S heat collecting type constant-temperature heating magnetic stirring apparatus under the power of 3kw by etching pit again
Agent is heated to 60 DEG C, then immerses mould steel sample to be corroded in metallographic etching agent, corrodes 8s to burnishing surface, at this time burnishing surface
It in silver gray, takes out, is then cleaned with deionized water to cleaning solution and be in neutrality, then with filter paper gently wiped clean, and with drying
Machine is in 70 DEG C of dry 20s.
Embodiment 4
The metallographic etching agent of the present embodiment, by picric acid, surfactant A, surfactant B and following volumes score
Raw material is made: 5 parts of acetic anhydride, 60 parts of methanol and 20 parts of water；Every 1ml methanol is corresponding to use 0.2g picric acid；The surface-active
Agent A is neopelex；The surfactant B is sodium sulfate of polyethenoxy ether of fatty alcohol；The picric acid, surface
Activating agent A and the mass ratio of surfactant B are 1:3:0.2.
The preparation method is the same as that of Example 1 for the metallographic etching agent of the present embodiment.
Embodiment 5
The metallographic etching agent of the present embodiment, by picric acid, surfactant A, surfactant B and following volumes score
Raw material is made: 4.5 parts of acetic anhydride, 60 parts of methanol and 25 parts of water；Every 1ml methanol is corresponding to use 0.2g picric acid；The surface is living
Property agent A be neopelex；The surfactant B is dodecanolyacylamine；The picric acid, surfactant
A and the mass ratio of surfactant B are 3:4:0.4.
The preparation method is the same as that of Example 1 for the metallographic etching agent of the present embodiment.
Embodiment 6
The metallographic etching agent of the present embodiment, by picric acid, surfactant A, surfactant B and following volumes number
Raw material is made: 4 parts of acetic anhydride, 70 parts of methanol and 30 parts of water；Every 1ml methanol is corresponding to use 0.3g picric acid；The surface-active
Agent A is neopelex；The surfactant B is nonylphenol polyoxyethylene ether；The picric acid, surfactant
A and the mass ratio of surfactant B are 6:4:0.3.
The preparation method is the same as that of Example 1 for the metallographic etching agent of the present embodiment.
Claims (10)
1. metallographic etching agent, it is characterised in that: by picric acid, surfactant A, surfactant B and following volumes number
Raw material is made: 3 ~ 5 parts of acetic anhydride, 60 ~ 75 parts and 20 ~ 40 parts of water of methanol；Every 1ml methanol is corresponding to use 0.2 ~ 0.4g picric acid；
The surfactant A is neopelex；The surfactant B is sodium sulfate of polyethenoxy ether of fatty alcohol, ten
At least one of dialkyl group alkylolamides, nonylphenol polyoxyethylene ether；The picric acid, surfactant A and surfactant B
Mass ratio is 1 ~ 8:3 ~ 6:0.2 ~ 0.5.
2. metallographic etching agent according to claim 1, it is characterised in that: the surfactant B is fatty alcohol polyoxy second
The mixture of alkene ether sodium sulfate, dodecanolyacylamine and nonylphenol polyoxyethylene ether.
3. metallographic etching agent according to claim 2, it is characterised in that: fatty alcohol polyoxyethylene ether sulphur in the mixture
The mass ratio of sour sodium, dodecanolyacylamine and nonylphenol polyoxyethylene ether is 0 ~ 5:0 ~ 10:0 ~ 10.
4. application of the metallographic etching agent as described in claim 1 in display steel in terms of carbide and/or crystal boundary.
5. application of the metallographic etching agent according to claim 4 in display steel in terms of carbide and/or crystal boundary, special
Sign is: changing colour the following steps are included: the steel with burnishing surface are immersed corrosion to burnishing surface in metallographic etching agent, after taking-up
It cleaned, dried.
6. application of the metallographic etching agent according to claim 5 in display steel in terms of carbide and/or crystal boundary, special
Sign is: metallographic etching agent is heated to after 60 ~ 100 DEG C again corroding steel immersion metallographic etchant.
7. application of the metallographic etching agent according to claim 6 in display steel in terms of carbide and/or crystal boundary, special
Sign is: etching time of the steel in metallographic etching agent is 3 ~ 10s.
8. application of the metallographic etching agent according to claim 5 in display steel in terms of carbide and/or crystal boundary, special
Sign is: the cleaning uses neutral liquid.
9. application of the metallographic etching agent according to claim 8 in display steel in terms of carbide and/or crystal boundary, special
Sign is: the neutral liquid is one of alcohol, acetone, water.
10. application of the metallographic etching agent according to claim 5 in display steel in terms of carbide and/or crystal boundary,
Be characterized in that: the drying is to spontaneously dry under drying or normal pressure；The temperature of the drying is 60 ~ 80 DEG C, and the time is 10 ~ 30s.
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| CN108362694B (en) * | 2018-01-16 | 2020-11-27 | 北京大学 | Method for rapidly detecting two-dimensional transition metal chalcogenide crystal boundary |
| CN109355661B (en) * | 2018-08-29 | 2021-04-09 | 东风汽车有限公司 | Corrosive agent for steel plate welding area, corrosion method and application |
| CN110118779A (en) * | 2019-05-13 | 2019-08-13 | 中天钢铁集团有限公司 | A kind of the dendrite corrosive agent and display methods of the heat resisting steel containing chromium |
| CN110174296A (en) * | 2019-06-12 | 2019-08-27 | 上海电气核电设备有限公司 | A kind of carbide display methods of nickel-base alloy metallographic structure |
| CN112903402B (en) * | 2021-01-21 | 2022-06-07 | 东北大学 | Cast dendrite corrosive for hot work die steel H13 |
| CN113866055A (en) * | 2021-09-01 | 2021-12-31 | 东方电气(广州)重型机器有限公司 | Method for detecting grain size of quenched and tempered steel |
| CN114184613A (en) * | 2021-12-07 | 2022-03-15 | 江苏天鼎检测科技有限公司 | Method capable of clearly displaying carbide |
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